FIELD: chemistry.
SUBSTANCE: invention relates to a method of preparing a trioxepane compound of formula (I) comprising less than 3.5 wt % of dialkyl peroxide based on the total amount of peroxides, the said process comprising steps of reacting a glycol compound of formula R3CHOH-CH2-C(CH3)2OH with hydrogen peroxide in the presence of an acid to form a glycol hydroperoxide, purifying the glycol hydroperoxide, reacting the purified glycol hydroperoxide with a ketone or aldehyde of formula R1R2CO in the presence of an acid to form the trioxepane compound, and purifying the trioxepane compound, wherein R1, R2 and R3 are independently selected from hydrogen and (C1-C20)-alkyl, (C3-C20)-cycloalkyl, (C6-C20)-aryl, (C7-C20)-aralkyl and (C7-C20)-alkaryl, where the said groups may include straight or branched alkyl groups, while two groups from R1-3 may bond to form a cycloalkyl ring; where optionally one or more substitutes for each R1-3 are selected from a group consisting of hydroxy, alkoxy, straight or branched alk(en)yl, aryloxy, halogen, carboxylic acid, ester, carboxy, nitrile and amido with the proviso that if R1 and R2 are both methyl groups, R3 is not hydrogen.
EFFECT: initiator compositions containing the so-prepared trioxepane compound are characterised by a high safe processing temperature combined with good crosslink efficiency.
10 cl, 29 ex
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Authors
Dates
2010-09-10—Published
2005-09-27—Filed